一种简单且通用的头空间GC-FID方法,用于准确量化药品中的挥发性氨基
Congchao You1, Tien Ho1, Victor Rucker1
1Analytical Development and Operations, Gilead Sciences, 333 Lakeside Drive, Foster City, CA 94404, USA. Lin.Wang@gilead.com.
Analytical methods : advancing methods and applications
|August 30, 2023
概括
一种新的头部气体染色法有效量化了制药中的残留挥发性氨基. 添加1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) 显著提高了对这些关键制药杂质的准确性和精度.
科学领域:
- 药品分析 药品分析
- 分析化学 分析化学
- 化学工程是化学工程的重要组成部分.
背景情况:
- 挥发性氨基在制药生产中至关重要,由于安全规定,需要严格控制最终产品中的残留物.
- 由于药品样本中的潜在矩阵相互作用和化学反应性,准确量化残留挥发性氨基是具有挑战性的.
- 现有的方法可能会与挥发性氨基和活性药物成分 (API) 之间的复杂相互作用作斗争.
研究的目的:
- 开发一种通用且准确的方法来量化制药产品中的残留挥发性氨基.
- 为了应对矩阵效应的挑战,并在挥发性氨基分析中分析反应性.
- 提高API中残留挥发性胺监测的可检测性,准确性和精度.
主要方法:
- 用火焰电离检测 (HS-GC-FID) 方法开发一个头空间气相色谱.
- 使用1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) 作为一种添加剂,以减轻高沸稀释剂中的矩阵效应.
- 采用DBU作为气色谱 (GC) 失活试剂,以最大限度地减少分析物吸附.
主要成果:
- 开发的HS-GC-FID方法成功分离了14种常用的挥发性氨基.
- 添加DBU显著提高了残留挥发性氨基的检测能力和准确性,特别是在像Ketoprofen®这样的酸性API中.
- 通过减少界面吸附,DBU作为GC消活试剂的应用提高了方法精度.
- 方法验证证明了可接受的线性,LOD,LOQ,稳定性,精度和稳定性.
结论:
- 一种简单且通用的HS-GC-FID方法与DBU添加剂提供了一个强大的解决方案,用于量化药品中的残留挥发性氨基.
- 使用DBU有效地克服了矩阵效应,并改善了对具有挑战性的挥发性胺分析的分析性能.
- 这种经过验证的方法为药品质量控制中的法规合规提供了可靠的结果.
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